Multiple chromatograph column heater unit



Jan. 16; 1968 R. K. SEVERS MULTIPLE CHROMATOGRAPH COLUMN HEATER UNITFiled Feb. 14, 1966 Figure 'IIIIIIIIIIIIIIIJ United States PatentOfilice 3,363,447 Patented Jan. 16, 1968 3,363,447 MULTIPLECHROMATOGRAPH COLUMN HEATER UNIT Richard K. Severs, Mount Prospect,Ill., assignor to Universal Bil Products Company, Des Plaines, 111., acorporation of Delaware Filed Feb. 14, 1966, Ser. No. 526,979 7 Claims.(Cl. 7323.1)

The present invention is directed to a multiple column heater unit andmore particularly to the design and construction of a heating unit whichprovides for the rapid substitution of one gas chromatograph column foranother in the oven section of the unit.

chromatograph columns, as used in a gas-liquid chromatography,liquid-liquid chromatography, and gas-solid chromatography, contain asuitable solid absorbent material in granular form to effect aseparation of a fluid stream or, alternatively, they utilize a thinliquid film held over the exposed surface of an inert support material.In either case, the fluid sample being analyzed is introduced into thecolumn in a suitable carrier fluid so that there is a selectiveadsorption or liquid partitioning to provide separations analogous todistillation. Also, in either type of separation, the continuous flow ofthe fluid stream provides for the sequential removal of components fromthe column and their passage to suitable detector means which can sensethe relative volatilities, molecular weights, or other properties ofsuch components.

In most analytical laboratories it is generally necessary to haveseveral chromatograph units in order to accommodate various types ofanalyses which must be run through different types of sizes of columns;however, in many instances it would be possible to use the same heateror oven section if it were possible to effect a rapid change over ofchromatograph columns and not have to wait for a cooling down of theentire heater unit. In other words, with a rapid substitution of onecolumn for another in an already hot oven section, there can be carriedout successive analysis operations without necessarily utilizing anentirely separate heating unit or chromatograph unit.

Thus, it may be considered a principal object of the present inventionto provide a multiple column heating unit which is constructed andarranged to provide for the rapid substitution of one column foranother.

It is a further object of the present invention to provide a heater unithaving accompanying movable column support means or end manifold meansfor holding a plurality of columns, where such support means is movablewith respect to the oven section of the unit and, in addition, movableWall sections are provided for the oven unit whereby there may be arapid substitution of one column for another into the interior thereof.

Broadly, the present invention may be considered to provide a multiplecolumn heating unit which provides for the selective insertion of onechromatograph column of a plurality thereof into the oven portion of theunit and comprises in combination, an elongated oven cham ber having aheat supply source for heating the interior thereof, elongated movableWall portions for such chamher, a plurality of spaced apart separatecolumns supported by and extending from movable end mounting means, withthe latter being positioned in combination with said heating chamber totranslate with respect thereto and in turn permit any one of saidplurality of columns to be positioned interiorly within said ovenchamber upon temporarily moving aside said wall portions of saidchamber, and attachment means at the ends of each of said plurality ofcolumns for the connection thereof to a gas supply line.

Generally, the heating chambers or oven sections utilized in connectionwith chromatograph analyzing equipment are of the electrical resistanceheater type of construction whereby there may be a close control of theheat output by suitable electrical control means. Also, presentconstructions generally provide for the placement of an open heater unitover a mounted chromatograph column or the insertion of one or morecoiled columns through the top of an oven chamber. In contrast, themultiple column heater unit, as provided by the present invention, isnormally arranged to be in a fixed position, normally as a horizontallyarranged heating chamber having combined therewith a movable columnsupporting means such that the transverse movement of the latter willpermit the simultaneous removal of one column and the insertion ofanother into the heating zone. In order to provide for the substitutionof columns it is of course necessary that one or more wall sections ofthe heating chamber be movable for the temporary opening of such chamberportion while the substitution of columns takes place. For example,opposing wall sections of an elongated oven section may be hingedlyattached to a remaining fixed portion of the oven unit whereby there maybe a temporary lifting of such hinged sections while the translatingmovement of the column support means takes place to substitute onecolumn for another within the central portion of the oven section.

Various types of movable support members may be utilized, as well asvarious types of movements provided, so as to effect the removal andinsertion of column sections. For instance, in one type of unit, theremay be a plurality of columns supported from at least one rotatingdisc-like support member such that the rotation of the latter around acentral axis will effect the movement of one column out of the ovensection and the introduction of another into it, as long as the columnsections are located at equal radial distances fromthe axis of rotationand at suitable spaced distances from one another to permit a finalpositioning of the new column within the central portion of the oven. Inanother instance, the plurality of chromatograph columns may be mountedto project between or perpendicularly outwardly from at least elongatedsupport means which in turn is movably mounted with respect to the ovensection so as to have translative movement across the end of the ovensection and thus provide for the removal of one column and thesubstitution of another from one unidirectional movement. Inasmuch asvarious sizes, lengths and configurations of packed columns are used inchromatograph analysis operations, it is not intended that the pluralityof columns mounted on the support means for any one improved multiplecolumn unit will be of the same size and type. In other words, eachmultiple column unit may have several sizes and types of packed columnsections whereby the proper translative movement of the support means,following the opening of the movable wall sections of the oven chamber,will permit the selective removal of one column and the substitution ofa different desired type into a still hot oven section.

Reference to the accompanying diagrammatic drawing and the followingdescription thereof will serve to illustrate a broad concept of thepresent invention as well as point out additional advantageous featuresin connection therewith.

FIGURE 1 of the drawing is a sectional elevational view of oneembodiment of a multiple column heating unit providing for the mountingof a plurality of separate chromatograph columns between rotatable endsupport members.

FIGURE 2 of the drawing is also a sectional elevational view, asindicated by the line 2-4 in FIGURE 1, indicating how the rotationaltranslative movement of the columns with respect to the oven portion ofthe unit permits the substitution of one column for another.

FIGURE 3 of the drawing indicates in a partial sectional view how aplurality of columns may be mounted from a single rotative disc-likesupport member, with the column sections fabricated to have theirrespective end portions terminate at the same end of the oven sectionand exteriorly of a single common support member.

FIGURE 4 of the drawing indicates diagrammatically still anothermodified form of a multiple column heating unit, where the variouscolumn sections being mounted perpendicularly from an elongatedrectangular column support means in turn designed and supported to movehorizontally with respect to the oven section.

Referring now particularly to FIGURES 1 and 2 of the drawing, there isshown a multiple column heating unit having a heating chamber or ovensection 1 supported by means of brackets 2 which in turn extend upwardlyfrom a suitable supporting base or stand 3. As best shown by FIGURE 2,the oven chamber 1 has elongated wall portions 1 which are hingedlyconnected to the fixed shell portion of oven 1 by hinges 4 so that bytemporarily raising such side portions 1 there can be a rapidsubstitution of a diiferent chromatograph column, into the heating zone.Each of the oven sections may be provided with suitable electricalresistance coil heating (not shown) which in turn is supplied withelectrical energy through supply lines indicated as 5. The electricalheating may of course be controlled by suitable monitoring orprogramming means that is apart of a complete chromatograph unit, sothat it is not intended to limit the present invention to any particulartype of electrical heating or control system.

A central axle 6 is shown extending between bearing means 7 in the endsof the stand 3 whereby there is an axial supporting means for rotatablecolumn supporting disc-like members 8. In this instance, the rotatablesupport members 8 operate in unison and are provided with an insulatingmaterial 9 on the interior faces thereof such that those portions whichrotate in an arc-like movement across the ends of the oven section 1will in effect serve as the end portions of the latter. Also, as bestshown in FIGURE 2, there are indicated a plurality of separate spacedapart chromatograph columns 16, 11, 12, 13, 14- and 15 which in turn arepositioned at equal radial distances outwardly from axle 6 and supportedbetween the spaced apart rotatable disc-like members 8. Each of thecolumns through will of course have suitable end connector means 16which will permit an easy connection to the tubing or lines which willpass a carrier gas suitable to accommodate a chromatograph sample of thegas to be analyzed in a gas-operation.

While the present drawing indicates the different columns 10 through 15as being of a similar size and construction, it may be noted that thisis merely for illustrative purposes and that such columns will normallybe of different sizes and of different configurations and may containdifferent types of solid adsorbents or of different liquid media ondifferent inert supports, whereby each column is capable of carrying outa specific type of chromatograph analysis on different gas samples. Apreferred construction for the multiple column unit also provided forthe exchange of difierent columns into the support members 8 wherebythey may be easily removed for repair or for substitution purposes. Forexample, column 12 is shown diagrammatically as being removable from thesupport members 8 by reason of being in turn supported from smallinsertable collar or bushing means 17 adapted to be held within notchedsections 17' provided from the edges of support discs 8. Set screws or'other locking means not shown may be used to hold the removable portions17 within the notched sections 17'.

In'the operation of the unit, at the end of any one analysis period itis desired to substitute a new column for a presently used chromatographcolumn, i.e., column 10 for another type, such as 11, then the side wallportions 1' of the oven chamber may be lifted and the support members 8rotated whereby the column 10 moves into the position of the column 15,as shown in the present FIGURE 2 while the column 11 then moves into theinterior of the heating chamber. After the proper positioning of thesubstitute chromatograph column, then the hinged oven sections 1 arepermitted to be lowered and clamped into place in any suitable manner,even while they are in a heated state. In a similar manner, any othercolumn of the plurality thereof may be rotated into the desiredpositioning in the oven section for a new analysis procedure by thetemporary lifting of the wall sections 1' and the proper rotation of thesupport members 8.

In FIGURE 3 of the drawing, there is indicated diagrammatically amodified construction and arrangement of the present invention which hasan oven section 18 being supported from a suitable bracket means 19 and20 and a column support plate or member 21 being rotatably mounted on anaxle 22. The support member 21 is provided with a plurality of spacedcolumns such as 23 and 25 which extend perpendicularly therefrom atspaced radial distances which will in turn provide proper positioningwithin the non-moving oven chamber 18. However, the columns in thisinstance are provided with tube connector means 24 on the projecting endportions thereof at one end of the heating section and on the exteriorface of support disc 21. Thus, the opposing end portion of the ovenchamber may be of a fixed permanent construction and the second opposingrotating support member can be eliminated, as compared with theconstruction shown in FIGURE 1 of the drawing. The substitution of onecolumn for another within the oven section of the unit is, however,carried out in the same manner as that set forth for the embodiment ofFIGURES 1 and 2, by utilizing an oven chamber which is provided withhinged or otherwise movable side wall sections permitting their beingtemporarily raised during that period where one column, such as 23, isreplaced with another column such as 25. Again, it may be pointed outthat the heating chamber 18, as shown, is merely diagrammatic and thatsuitable electrical resistance heating coils, or the like, may beprovided around the interior wall portions thereof and a suitable powersupply source connected therewith in order to provide adjustable heatingfor such chamber. However, in the interest of simplicity, the electricalheating means and heat control means have not been shown in the presentdiagrammatic drawing.

In the modified design shown in FIGURE 4 of the drawing, there isindicated an oven unit 26 having movable wall sections 27 and 27', whichlike the other heating ovens may be suitably provided a heating sourcenot shown. The oven chamber 26 is indicated as being supported bybracket means 28 which in turn extends from a base 29. The latter isshown as being provided with notch or track means 30 to accommodateroller support means 31 on the bottom of a horizontally movable columnsupport means 32. The latter is of an elongated rectangular designadapted to hold a plurality of chromatograph columns 33, 34, 35 and 36in a common horizontal plane and at spaced positions which will providefor centering only one of the columns within the interior of the ovensection 26 at any one time. The several columns 33 through 36 may extendthrough opposing spaced apart end support plates, such as 32., or theymay be held so as to project outwardly and perpendicularly from theinside face of a single movable support means 32 provided along only oneend of the oven chamber 26.

In effecting the substitution of one chamber for another in the heatingchamber 26, the wall sections 27 and 27 shall be temporarily raised orotherwise moved from between the spaced apart columns whereby thelateral or translative movement of the support means 32 with respect tothe oven 26 will cause the removal of one column and the substitution ofanother. After the proper centering of the replacement column within theoven section 26, the wall sections 27 and 27' may be dropped to theirclosed positions and clamped or otherwise held in place during theperiod of the next gas analysis procedure.

Again it may be pointed out, that the various columns 33 through 36 maybe of entirely different sizes and configurations, or they containdiflerent types of solid adsorbents or liquid film materials on suitableinert mediums whereby entirely different gas analysis procedures may becarried outwith each of the separate column sections. As with the otherpreviously described embodiments, there is no need to wait for an ovenchamber cooling off period to effect a substitution of columns inasmuchas all that is required for the change is the rapid lifting of themovable Wall sections, the disconnection of end connector means for theused column section, and the connecting of the gas lines to thereplacement column section.

In each of the diagrammatic embodiments of the accompanying drawingthere have been shown single coils as providing the various differentchromatograph columns for placement in the heating section of the unit;however, it may be noted that many of the modern type chromatographunits make use of dual coil arrangements to serve as any one column in agas analysis procedure. Thus, it is not intended to limit the presentimproved multiple column construction and arrangement to the use ofsingle coils for each column, inasmuch as parallel coil type columns mayreadily be provided for and embodied into the present multiple columnconcept. In other words, dual column arrangements may be provided forwithin each oven section at any one time and for any one gas analysisprocedure. Also, the column ends and gas line connector means may beprovided to terminate exteriorly of one support member or at onemanifold means at one end of the oven section or, in an alternativemanner, there may be connections to the separate ends of the coils orcolumns from the opposing ends of the oven section and exteriorly ofspaced apart support members or manifold means.

I claim as my invention:

1. A multiple column heating unit providing for the selective insertionof one chromatograph column of a plurality thereof into the oven portionof the unit, which comprises in combination, an elongated oven chamberhaving a heat supply source for heating a column therein, elongatedmovable wall portions for such chamber providing for the replacement ofa column therein, a plurality of columns extending from end mountingmeans, with the latter being positioned in combination with said ovenchamber to translate with respect thereto and in turn permit any one ofsaid plurality of columns to be positioned interiorly within said ovenchamber upon temporarily moving aside said wall portions of saidchamber, and attachment means at the ends of each of said plurality ofcolumns for the connection thereof to a gas supply means.

2. The multiple column heating unit of claim 1 further characterized inthat the columns comprise more than one size and type where-by theplurality thereof for said unit provide for a rapid change over ofcolumns to permit a different gas analysis utilizing the same heatedoven chamber.

3. The multiple column heating unit of claim 1 further characterized inthat said oven chamber has opposing hinged wall sections whereby theremay be lateral removal and insertion of one column for another withinsaid chamber.

4. The multiple column heating unit of claim 1 further characterized inthat said plurality of columns are mounted perpendicularly outwardlyfrom at least one rotating disc-like support member at equal distancesfrom the center of rotation thereof, with such distances providing forthe locating of each of the columns interiorly within a fixedlypositioned oven chamber, whereby upon the temporary removal of ovenchamber wall sections and upon the rotation of the support means therewill be the removal of one column out of said oven chamber and theplacement of a different column into the interior thereof.

5. The multiple heating unit of claim 4 still further characterized inthat the plurality of said columns being supported from the rotatingsupport means have their end sections terminating exteriorly of thelatter at one end of the oven chamber.

6. The multiple column heating unit of claim 4 still furthercharacterized in that there are two spaced apart rotatable disc-likesupport means for said columns and such means are positioned to provideend closures for the oven chamber while being movable across each endand said plurality of columns extend longitudinally between said twoopposing rotatable support means with end connecting means providedexternally of the opposing support means.

7. The multiple heating column of claim 1 further characterized in thatsaid end mounting means holding said plurality of columns is of arectangular configuration with said columns being supported therefrom ina spaced parallel arrangement and said end mounting means has movablesupporting means arranged to move the mounting means across at least oneend portion of said oven chamber, such that upon the temporary liftingof wall sections of the latter there may be a removal of one column andthe insertion of a different column within the oven chamber of the unit.

References Cited UNITED STATES PATENTS 1,966,949 7/1934 Goldstein2l9-385 2,234,499 3/1941 McAllister 23-254 3,139,745 7/1964 Sievers etal. 73-23.1 3,201,921 8/1965 Heyes 386 XR 3,213,596 10/1965 Gill 73-23.1XR 3,248,517 4/1966 Vranken 219-388 XR 3,290,482 12/1966 Dodd et a173-2311 XR FREDERICK L. MATTESON, JR., Primary Examiner. A D. HERRMANN,Assistant Examiner.

1. A MULTIPLE COLUMN HEATING UNIT PROVIDING FOR THE SELECTIVE INSERTIONOF ONE CHROMATOGRAPH COLUMN OF A PLURALITY THEREOF INTO THE OVEN PORTIONOF THE UNIT, WHICH COMPRISES IN COMBINATION, AN ELONGATED OVEN CHAMBERHAVING A HEAT SUPPLY SOURCE FOR HEATING A COLUMN THEREIN, ELONGATEDMOVABLE WALL PORTIONS FOR SUCH CHAMBER PROVIDING FOR THE REPLACEMENT OFA COLUMN THEREIN, A PLURALITY OF COLUMNS EXTENDING FROM END MOUNTINGMEANS, WITH THE LATTER BEING POSITIONED IN COMBINATION WITH SAID OVENCHAMBER TO TRANSLATE WITH RESPECT THERETO AND IN TURN PERMIT ANY ONE OFSAID PLURALITY OF COLUMNS TO BE POSITIONED INTERIORLY WITHIN SAID OVENCHAMBER UPON TEMPORARILY MOVING ASIDE SAID WALL PORTIONS OF SAIDCHAMBER, AND ATTACHMENT MEANS AT THE ENDS OF EACH OF SAID PLURALITY OFCOLUMNS FOR THE CONNECTION THEREOF TO A GAS SUPPLY MEANS.